Title:
Atomic Layer Deposition As A Method Of Fine Tuning The Surface Chemistry Of Oxide Materials
Atomic Layer Deposition As A Method Of Fine Tuning The Surface Chemistry Of Oxide Materials
Author(s)
Yom, Typher
Advisor(s)
Losego, Mark D.
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Abstract
Atomic layer deposition (ALD) is a vapor-phase synthesis method in which a material is deposited onto a surface with precise atomic thickness. Through ALD, ultra-thin monolayers of oxide materials can be deposited onto powders, creating mixed oxide surfaces with tunable surface chemistries, enabling their usefulness towards catalytic processes in the petrochemical and fine chemical industries. ALD holds an advantage over typical solution-phase methods of creating mixed oxide materials due to the latter’s difficulty in controlling the surface composition, making analysis difficult. However, if we can better understand the interactions of the surface in solution, it can be used to design more effective catalysts. One way to observe this is by studying the zeta potential of the surface, which is directly correlated with surface charge and is a product of these acid-base interactions at the interface. Each material can be identified using the isoelectric point, which is the point at which the zeta potential/net surface charge is zero. For mixed metal oxides, their isoelectric points were calculated in the literature to be the summation of each individual component’s isoelectric point multiplied by its surface coverage. However, this calculation assumes that the components do not interact with each other when mixed. In order to investigate this discrepancy, we used ALD to deposit thin layers of titanium oxide onto silicon oxide powders. If we were to assume the equation used in the literature, we can assume that one single monolayer over the surface would be sufficient to convert the isoelectric point from that of silicon oxide to that of titanium oxide. However, our results have indicated that the isoelectric point did not reach that of titanium oxide until multiple monolayers were deposited, indicating that a different model/equation must be utilized to better elucidate the surface behavior. Additionally, during these studies of the isoelectric point, we have formulated an equation that can correlate the thickness of ALD-deposited films with the material’s relative atomic percent. This equation was created by assuming that the shape of the particle + film retains its shape, and therefore its volume formula, allowing it to work for ultra-thin films, but not for much thicker films. Finally, this thesis highlights the importance of being mindful of the precursor used for powder ALD: precursors like TiCl4 can create byproducts like HCl from the reactor walls and the powder itself. These byproducts can then adsorb onto the powder surface, which can block film growth or affect the pH of the resulting solution when the powder is dispersed in water. Extra measures, such as a double dose or a post-process washing step, were implemented, and should be used when performing powder ALD.
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Date Issued
2023-12-05
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